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Butanal → 1-(But-1-enyl)pyrrolidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Butanal | HCID 261 | — |
| 反応物 | 2-Pyrrolidone | HCID 12025 | — |
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(But-1-enyl)pyrrolidin-2-one | HCID 580170 | — |
反応手順
A solution of 2-pyrrolidone (50 g, 0.588 mol), butanal (42.4 g, 0.588 mol) and P2O5 (2 g, 0.014 mol) in 300 ml toluene, were refluxed together for 10 hours using Dean-Stark apparatus to collect liberated water. The resulting solution was cooled and washed with 5% solution of sodium bicarbonate and dried over anhydrous sodium sulphate. After removing the solvent under reduced pressure, 1-(but-1-enyl) pyrrolidin-2-one (I) was obtained by distillation as a liquid. (68.2 g, 83.2%). 1H NMR (CDCl3): δ 1.02 (3H,t), 2.03-2.15 (4H, m), 2.45 (2H, t), 3.5 (2H, t), 5.01 (1H, m), and 6.85 (1H, d). 13C-NMR (CDCl3): δ 172.52, 122.91, 113.8, 45.09, 31.07, 23.03, 17.27, and 14.27. IR: 2962, 2930, 1698, 1663, 1253 Cm−1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08389733B2 |
| 出典データセット | uspto-grants-2013_03 |
| ORD ID | ord-6cf4663b96a54497b94c63eeb477f61e |
| 出典メモ | uspto-grants-2013_03 |